US4686052A - Stabilized fracture fluid and crosslinker therefor - Google Patents
Stabilized fracture fluid and crosslinker therefor Download PDFInfo
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- US4686052A US4686052A US06/753,214 US75321485A US4686052A US 4686052 A US4686052 A US 4686052A US 75321485 A US75321485 A US 75321485A US 4686052 A US4686052 A US 4686052A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/005—Crosslinking of cellulose derivatives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S507/00—Earth boring, well treating, and oil field chemistry
- Y10S507/903—Crosslinked resin or polymer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S507/00—Earth boring, well treating, and oil field chemistry
- Y10S507/922—Fracture fluid
Definitions
- This invention pertains to stabilized aqueous zirconium and titanium crosslinking compositions for use with solvatable polysaccharides to form stabilized crosslinked gels. This invention also pertains to processes for using such gels as fracture fluids for fracturing subterranean formations.
- the present invention includes a process for fracturing a subterranean formation penetrated by a wellbore which comprises the steps of:
- Hydraulic fracturing is a term that has been applied to a variety of techniques used to stimulate the production of oil, gas and other fluids from subterranean formations.
- suitable fracturing fluid is introduced into a subterranean formation by way of a wellbore under conditions of flow rate and pressure which are at least sufficient to create and/or extend a fracture into a desired part of the formation.
- the fracturing fluid normally carries with it a proppant (e.g., sand, bauxite, etc.) which is forced into the fracture itself and keeps the broken formation from closing down upon itself once the pressure is released.
- a proppant e.g., sand, bauxite, etc.
- Aqueous gels are usually prepared by blending a polymeric gelling agent with an aqueous medium.
- the polymeric gelling agent of choice is a solvatable polysaccharide.
- These solvatable polysaccharides form a known class of compounds which include a variety of natural gums as well as certain cellulosic derivatives which have been rendered hydratable by virtue of hydrophilic substituents chemically attached to the polymer backbone.
- the solvatable polysaccharides therefore include galactomannan gums, glucomannan gums and cellulose derivatives.
- polymers examples include guar, carboxyalkyl guar, hydroxyalkyl guar, and carboxyalkyl hydroxyalkyl guar, galactomannan gums, glucomannan gums, xanthan gums, and the like.
- the solvatable polysaccharides have a remarkable capacity to thicken aqueous liquids. Even small amounts are sufficient to increase the viscosity of such aqueous liquids from 10 to 100 times or more. In many instances, the thickened aqueous liquid has sufficient viscosity to carry the proppant during the course of the fracturing process and represents a satisfactory fracturing fluid. In other instances, it is necessary to crosslink the polysaccharide in order to form a gel having sufficient strength and viscosity to carry out the proppant. A variety of crosslinkers have been developed to achieve this result.
- the borate ion has been used extensively as a crosslinking agent for hydrated guar gums and other galactomannans to form aqueous gels used in fracturing and other areas.
- Kern described a crosslinked system in U.S. Pat. 3,058,909 which was used extensively in the oil and gas industry as a fracturing fluid.
- a fracturing process which comprised crosslinking, guar-containing compositions on-the-fly with borate ions was described by Free in U.S. Pat. No. 3,974,077.
- the borate-crosslinked systems require a basic pH (e.g., 8.5 to 10) for crosslinking to occur.
- Chrisp and Tiner et al. each described titanium crosslinkers in which the "amine" portion of the crosslinker was a residue of triethanolamine.
- Chrisp in U.S. Pat. No. 3,301,723 at column 5, line 60 identified the crosslinker as titanium-triethanolamine chelates.
- Tiner er al. in U.S. Pat. No. 3,888,312, column 3 at lines 32-35 identified the compound as bis(triethanolamine)bis(isopropyl)titanium (IV).
- Chrisp and Tiner at el. also disclosed a wide variety of other compounds in which the "anion" portion of the molecule was something quite different than the triethanolamine residue (e.g. chloride). Chrisp in U.S. Pat. No.
- Tiner et al. likewise taught that the crosslinking ability of their titanium crosslinking agent depended upon the presence of titanium in the +4 oxidation state and that the "anion" portion of the molecule could be carried. This broad teaching in Tiner et al. is once again analogous to the teaching in Chrisp.
- solvatable polysaccharides are typically crosslinkable in a basic aqueous medium (at a pH above 7) by a wide variety of organometallic compounds containing titanium or zirconium in a +4 oxidation (valence) state. These solvatable polysaccharides have a remarkable capacity to thicken aqueous liquids and thus to form gels.
- the crosslinked aqueous-base polysaccharide gels have been widely used as hydraulic fracture fluids for injection into subterranean formations to enhance the production of fluids therefrom. Hydraulic fracturing is a term applied to a variety of techniques used to stimulate the production of oil, gas and other fluids from subterranean formations.
- a suitable fracture fluid is introduced into a subterranean formation by way of a wellbore under conditions of flow rate and pressure which are at least sufficient to create and/or extend a fracture into a desired part of the formation.
- the fracture fluid normally carries with it a proppant (e.g., sand, bauxite, glass beads, etc.) which is forced into the fracture and keeps the broken formation from closing down upon itself once the pumping pressure is released.
- a proppant e.g., sand, bauxite, glass beads, etc.
- the organometallic crosslinking agents containing titanium or zirconium in a +4 valance state likewise form a known class of compounds.
- a preferred class of zirconium crosslinking agent is disclosed in British Pat. No. 2,108,122 (Kucera), the disclosure of which is incorporated herein by reference.
- This class of crosslinking agents is prepared by reacting zirconium tetraalkoxides with alkanolamines under essentially anhydrous conditions.
- Other zirconium and titanium crosslinking agents are described, for example, in U.S. Pat. No. 3,888,312 (Tiner et al.), U.S. Pat. No. 3,301,723 (Chrisp), and U.S. Pat. No.
- aqueous solutions of zirconium and titanium crosslinking agents for solvatable polysaccharide solutions are stabilized by, and the functional effectiveness of such crosslinking agents is retained at least in significant part by, the inclusion of a small but stabilizing amount of an alkanolamine.
- These stabilized compositions are new compositions of matter.
- a solvatable polysaccharide in a basic aqueous medium with the stabilized crosslinker solutions is also a new composition of matter which can be utilized in hydraulic fracturing as an improved fracture fluid. It has surprisingly been found that the crosslinked fluid is unusually resistant to shear degradation under conditions of use at elevated temperatures.
- Other conventional fracture fluid additives e.g., proppant, gel stabilizers, or viscosity breakers
- proppant e.g., gel stabilizers, or viscosity breakers
- the organometallic crosslinking agents containing titanium or zirconium in a +4 oxidation valance state form a known class of compounds, any member of which can be used herein provided the selected compound crosslinks solvatable polysaccharides in an aqueous medium at a basic pH.
- Those organometallic compounds containing one or more alkanolamine liqands are preferred in the present invention, and those compounds containing one or more ethanolamine (mon-, di- or triethanolamine) liqands are most preferred.
- the zirconium crosslinkers are preferred in many instances because of their "delayed” or "retarded" crosslinking reactivity.
- This delayed activity is useful in fracturing operations because it lets the operator formulate and pump the uncrosslinked fracture fluid while it has a relatively lower viscosity; this means lower hydraulic horsepower is required to pump the fluid, which means lower costs.
- the delayed systems are usually designed to crosslink while the fluid is being pumped through the wellbore tubing and/or as the fracture fluid enters the fracture. The velocity of the fracture fluid becomes lower as the fluid enters the fracture and the viscosity of the fluid must then be adequate to hold the proppant in suspension until the pumping (facturing) operations are complete.
- the zirconium crosslinkers described by Kucera are a most preferred class of crosslinkers for use herein.
- the organometallic crosslinkers are dissolved in water and the aqueous solution thereof stabilized by adding at least one alkanolamine to the solution; the resultant solution is referred to herein as a stabilized crosslinker solution or composition.
- This stabilized crosslinker composition is combined in small but effective crosslinking amounts with an aqueous solution of solvatable polysaccharides so as to form first a crosslinkable fluid and then a crosslinked gel.
- This gel is useful as a fracture fluid in fracturing a subterranean formation penetrated by a wellbore using conventional techniques.
- the stabilized hydraulic fracturing fluids of the present invention are introduced into the formation through the wellbore at a flow rate and pressure sufficient to create, reopen and/or extend a fracture in the formation.
- This may be accomplished by using either a batch mix or continuous mix technique.
- the solvatable polysaccharide solution (and optional additives) is pre-mixed in a tank.
- the stabilized crosslinker solution is then injected into a flowing stream of the aqueous polysaccharide solution and the combined fluid is pumped down the wellbore.
- the solvatable polysaccharide is added directly to a flowing stream of aqueous fluid and the crosslinker solution is added to this flowing stream at or near the wellhead after allowing sufficient residence time in the tubular goods for the polysaccharide to hydrate.
- Specific details of the hydraulic fracturing process will be known to those skilled in art, the novel aspect of which, in accordance with the present invention, is the utilization of a stabilized crosslinker composition in formulating an improved fracture fluid.
- Crosslinking compositions in accordance with the present invention can also be utilized with solvatable polysaccharide solution including other additives such as viscosity modifiers or breakers, typically including alkali (i.e. alkali metal or ammonium) persulfate, as disclosed in U.S. Pat. No. 4,250,044; gel stabilizers, such as the alkali thiosulfate and ammonium thiosulfate, and methanol; proppant, such as sand, bauxite, glass beads, etc.
- viscosity modifiers or breakers typically including alkali (i.e. alkali metal or ammonium) persulfate, as disclosed in U.S. Pat. No. 4,250,044
- gel stabilizers such as the alkali thiosulfate and ammonium thiosulfate, and methanol
- proppant such as sand, bauxite, glass beads, etc.
- the solvatable polysaccharides with which the present invention may be used, particularly for applications such as fracture fluid, are those having a molecular weight of at least about 100,000. Normally polysaccharide molecular weights of about 1-5 million are preferred.
- the known class of solvatable polysaccharides referred to above includes, for example, locust bean gum and guar gum, as well as other galactomannan and glucomannan gums, such as those from endosperms of seeds of other leguminous plants such as the sennas, Brazilwood, Tera, Honey locust, Karaya gum and the like.
- hydroxyethylguar hydroxypropylguar, carboxyethylhydroxyethylguar, carboxymethylhydroxypropylguar, and the like.
- Cellulose derivatives containing only hydroxy/alkyl groups e.g. hydroxyethylcellulose
- Guar gum, hydroxypropylguar, and locust bean gum are preferred polysaccharides for use in the present invention and hydroxypropylguar is the most preferred gum based upon its commercial availability and desirable properties.
- the solvatable polysaccharides can be used individually or in combination; usually, however, a single material is used.
- a preferred subclass of polysaccharides includes those polysaccharides which have a plurality of vicinal hydroxyl groups oriented sterically in a cis configuration. This includes galactomannan gums, glucamannon gums, and other such hydrophilic vegatable gums, and certain cellulose derivatives.
- the solvatable galactomannan gums and glucomannan gums are, of couse, naturally occurring.
- the cellulose derivatives are reaction products of cellulose with compounds which render the cellulose derivatives solvatable and crosslinkable by the chemical attachment of hydrophilic constituents to the cellulose backbone. For example, the reaction product of alkali cellulose with sodium chloroacetate gives a product known as carboxymethylcellulose.
- derivatives of the naturally occurring gums can be prepared and used herein so long as the derivatives thereof are solvatable and crosslinkable.
- the reaction product of guar gum with propylene oxide gives a derivative known as hydroxypropylguar which is particularly useful herein.
- the amount of alkanolamine used in the present invention can be varied, but generally the molar ratio of alkanolamine to titanium or zirconium is at least about 15 to stabilize aqueous crosslinker solutions, and at least about 42 to provide shear stability for the crosslinked gels at elevated temperatures (e.g., above about 200° F.).
- the solvatable polysaccharides are normally blended with a solvent such as water or an aqueous medium (e.g., aqueous methanol, ethanol, or 1 to 3% HCl) to form an uncrosslinked gel as a first step.
- a solvent such as water or an aqueous medium (e.g., aqueous methanol, ethanol, or 1 to 3% HCl)
- the rate of solvation of the particular polysaccharide vary with the particular combination of solvent and polysaccharide chosen. Because of this, it is generally advantageous to preblend the polysaccharide with the particular solvent medium to obtain a smooth uniform gel before blending in the crosslinker.
- a "gel” is a homogenous or substantially homogeneous solid/liquid mixture in which the solid particles vary in size down to substantially colloidal dimensions and the mixture is capable of resisting a finite shearing force, such resistance to shearing is usually evidenced by viscosity measurements.
- the amount of solvatable polysaccharide that is used in making a gel can vary in the instant invention. Usually only a small amount of polysaccharide is required because of the high efficiency that such polysaccharides display in thickening aqueous media. For most applications, satisfactory gels are made by adding the solvatable polysaccharide in amounts up to about 5 weight percent, based on the weight of the aqueous liquid. Preferred amounts of polymer generally range from about 0.3 to about 3 weight percent.
- the aqueous medium is usually water or a water/alcohol mixture.
- the aqueous media can of course contain other additives which increase the rate of solvation of the polymer or perform some other desirable function.
- the aqueous media may contain buffering agents, acids or bases, iron control agents, bactericides, diesel oil, chemical breakers which break the crosslinked polymers in a controlled manner, stabilizers, surfactants or formation control agents.
- Such additives may be added to the aqueous gel before or after the polysaccharide is solvated, but generally are added after.
- the gels formed by blending the solvatable polysaccharide with an aqueous media are uncrosslinked gels.
- Such gels have an increased viscosity but they are substantially weaker than the crosslinked gels and the uncrosslinked gel structure can be broken (rather easily in most instances) by temperature, high shear, and/or the presence of dissolved electrolytes.
- the stabilizing effect of the alkanolamines on an aqueous zirconium/titanium crosslinking composition and on a crosslinked polysaccharide composition has been demonstrated by the following examples and comparative tests.
- a 10 mL Control Sample of a zirconium/triethanolamine crosslinking agent in propanol media (prepared by reacting zirconium propoxide with triethanolamine in accordance with the above-referenced Kucera British patent) was added to 40 mL of deionized water prewarmed to test temperature.
- a series of tests were conducted on this Control Sample by maintaining solution prepared in this manner in water baths at various test temperatures for several hours. At regular intervals an aliquot of the crosslinker solution was withdrawn from the bath and its crosslinking reactivity evaluated by the following general procedure:
- HPG hydroxypropylguar
- reaction vessel II Place the reaction vessel in a 140° F. water bath and stir the contents vigrously with a metal spatula until it becomes significantly harder to stir and mounding of the resulting gel occurs with stirring. This is designated as the thickening or crosslink time.
- a Test Sample of the present invention was then prepared by combining 10 mL of the Control Sample with 11 mL of triethanolamine and 29 mL deionized water. This provided a trialkanolamine to zirconium molar ratio of about 25:1 versus a ratio of about 4.7:1 in the Control Sample.
- Crosslink tests were then performed the same as for the control sample except that the gel pH was not adjusted (since the additional triethanolamine performed that function) and tests were conducted at higher temperature. Approximate crosslink times are reported below:
- crosslinker compositions stabilized in accordance with the present invention confirmed its advantages under conditions of use. In numerous instances where crosslinker compositions in accordance with the present invention were mixed and held at elevated ambient temperatures for several hours or overnight before use the mixture maintained its reactivity as evidenced by surface crosslinking tests and by successful treatment of the well. Crosslinker compositions containing the same active crosslinking agents which were previously in use were not similarly stable. It was necessary to discard and remix them if held more than 8 hours at 80° F. or more than 2 hours at 100° F.
- Heat-induced gel breakdown was tested as an indication of gel stability by using an HPG based gel system (0.48% or 40 pounds per 1000 gallons HPG in water).
- This gel also contained approximately 1% potassium chloride, an antifoam agent, bactericide, a surfactant and a conventional gel stabilizer as used in a commercial fracture fluid.
- Crosslinker solution was added through a mixer valve from a positive displacement syringe pump. The polysaccharide solution was pumped at 80 mL per minute and the crosslinker solution at 14.4 mL per hour. For the control, sodium carbonate was added to bring the pH to 9.5. This fluid was pumped through 360 feet of 0.08 inch I.D.
- the crosslinker composition was a solution of 20% crosslinking agent, prepared as described in Example 1 and 80% water.
- the stabilized compositon of the present invention was produced either by adjusting the pH of the polysaccharide solution to 9.25 with triethanolamine and using a crosslinker solution comprising 20% crosslinking agent and 80% water described in Example 1 or by preparing a solution comprising 21-22% triethanolamine, 58-59% water, and 20% crosslinking agent.
- a shear rate/shear stress scan (typically referred to as a ramp) from 85-511 reciprocal seconds (or 100-600 RPM with R1B5 cup and bob combination) was run 3 minutes after loading the Fann device. The heated baths were then raised to enclose the cup and the temperature of the test fluid raised to 275° F. Additional ramps were run at times of 0, 0.5 hour and 1 hour, and hourly thereafter. The results are shown in Table II.
- crosslinking compositions further including additional triethanolamine in the amounts of 7, 9, 10, and 11 mL (alkanolamine to zirconium ratios of 17.7, 21.5, 23.3 and 25.2 respectively).
- the 9, 10 and 11 mL TEA compositions showed little increase in crosslink time as the crosslinking composition aged up to six hours at 120° F. Specifically, the crosslink time for these compositions increased from about one minute to about two-and-one-half minutes (for the 11 mL TEA sample).
- the sample with 5 mL TEA composition showed a crosslink time increase to 7 minutes and the 7 mL TEA sample to 4 minutes crosslink time. This significant difference is believed to indicate that an alkanolamine to zirconium ratio of about 15 is sufficient to produce a discernible stabilizing effect in accordance with the present invention.
- a test conducted with 0.48% guar gum solutions also demonstrates the unexpected stability imparted to the crosslinked polysaccharide by the use of triethanolamine in accordance with the present invention.
- the test procedure was the same as in Example 1 except that the test temperature was 200° F.
- the guar solution pH was adjusted to 9.25 with sodium carbonate.
- the test guar solution pH was brought to the same level with 0.8 mL/1000 mL (i.e., 0.8 gal/1000 gal triethanolamine).
- the crosslinker in both cases was a 20% aqueous solution of the crosslinking agent described in Example 1. Results are presented in Table III below
- the crosslinked fluids are useful as fracturing fluids.
- a well was treated according to the present invention.
- the fracturing fluid utilized both the stabilized crosslinker and the high temperature gel stabilizer.
- Bottom hole static temperature (BHST) of the well was 295° F. and the perforated interval was at a depth of 11,452 to 11,486 feet.
- the fracturing fluid consisted of 55,00 gallons of 2% KCl water with 50 lb/1000 gal of HPG, 10 lb/1000 gal of ammonium thiosulfate stabilizer and appropriate amounts of the customary additives for fracturing fluids (bactericide, surfactants, clay stabilizer, silica flour fluid loss additive).
- Crosslinker was mixed in two separate batches--one for the pad fluid and one for the proppant stages.
- Crosslinker for the pad stage consisted of 20 gallons of crosslinking agent cited in the control in Example 1, 48 gallons of 85% triethanolamine and 15% water, and 32 gallons of water.
- Crosslinker for proppant stages consisted of 29 gallons of the same crosslinking agent, 69 gallons of the triethanolamine-water mixture, 47 gallons of water and 14 pounds borax (added to enhance early viscosity). Both crosslinker mixtures were added with a liquid additives pump on the discharge side of the blender at a rate such as to add 3.5 gallons crosslinker solution for every 1000 gallons of fracturing fluid. 20,000 gallons of pad fluid was followed by 35,000 gallons of proppant laden fluid, all fluids pumped at a rate of 10 barrels per minute (BPM). 80,000 lbs of 20/40 mesh Ottawa sand and 15,000 lbs of 20/40 mesh intermediate strength proppant were added during the proppant stages.
- Borax is preferably added to the present fluids (aqueous gel compositions) in amounts of from about 0.1 to about 0.7 pounds per 1000 gallons of aqueous gel compositions; and is most preferably added in amounts of from about 0.25 to about 0.5 pounds per 1000 gallons.
Abstract
Description
TABLE I ______________________________________ Age Control at Control at Test Sample Test Sample (hrs) 85-90° F. 100° F. at 100° F. at 120-122° F. ______________________________________ 0 1 1 to 2 1.5 1.5 1 to 2 5 2 -- 1 2 5 to 6 2 to 2.5 2.5 to 3 2 5 8 2 to 2.5 2.5 to 3 3 5 to 7 10 2 to 2.5 2.5 to 3 4 9 13 2.5 to 3 2.5 to 3 5 10 to 11 -- -- 3 19 -- -- 2.5 to 3 -- 24 -- -- -- 3 to 3.5 ______________________________________
TABLE II ______________________________________ FANN 50C DATA AT 275° F., DUPLICATE TESTS CONTROL TEST Viscosity Viscosity Time (at 170 Time (at 170 (hrs) sec -1) n' K' (hrs) sec -1) n' K' ______________________________________ Before 51 .283 .042 Before 67 .455 .023 Heat Heat 0 86 .586 .015 0 117 .656 .014 0.5 86 .596 .014 0.5 149 .620 .022 1 92 .585 .016 1 150 .608 .024 2 96 .581 .017 2 154 .596 .026 3 94 .574 .018 3 146 .599 .023 4 134 .603 .022 Before 67 .472 .021 Before 59 .482 .018 Heat Heat 0 125 .844 .006 0 104 .631 .014 0.5 100 .654 .013 0.5 128 .611 .020 1 99 .641 .013 1 133 .601 .022 2 82 .671 .009 2 121 .621 .018 3 68 .698 .007 3 113 .627 .016 4 104 .637 .014 ______________________________________
TABLE III ______________________________________ Time (hrs) Control Test 1 Test 2 ______________________________________ Before heat 83 87 90 0 64 126 123 1 29 107 100 2 26 93 83 3 25 91 77 4 24 77 69 ______________________________________
Claims (17)
R--N--(CH.sub.2 --CH(OH)--R').sub.2
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/753,214 US4686052A (en) | 1985-07-08 | 1985-07-08 | Stabilized fracture fluid and crosslinker therefor |
CA000499018A CA1269093A (en) | 1985-07-08 | 1986-01-06 | Stabilized fracture fluid and crosslinker therefor |
EP86201144A EP0208373B1 (en) | 1985-07-08 | 1986-06-30 | Stabilized fracture fluid and crosslinker therefor |
DE8686201144T DE3688303T2 (en) | 1985-07-08 | 1986-06-30 | STABILIZED FRACTURING LIQUID AND YOUR NETWORKER. |
NO862735A NO862735L (en) | 1985-07-08 | 1986-07-07 | REPAIR FOR CROSS-BONDING A SOLUBLE POLYSACCHARIDE, FOR USE IN THE FRACTURING OF A SUBSTANCES. |
US06/929,567 US4780223A (en) | 1985-07-08 | 1986-11-10 | Stabilized fracture fluid and crosslinker therefor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US06/753,214 US4686052A (en) | 1985-07-08 | 1985-07-08 | Stabilized fracture fluid and crosslinker therefor |
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US06/929,567 Division US4780223A (en) | 1985-07-08 | 1986-11-10 | Stabilized fracture fluid and crosslinker therefor |
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US4686052A true US4686052A (en) | 1987-08-11 |
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US06/753,214 Expired - Lifetime US4686052A (en) | 1985-07-08 | 1985-07-08 | Stabilized fracture fluid and crosslinker therefor |
US06/929,567 Expired - Lifetime US4780223A (en) | 1985-07-08 | 1986-11-10 | Stabilized fracture fluid and crosslinker therefor |
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US06/929,567 Expired - Lifetime US4780223A (en) | 1985-07-08 | 1986-11-10 | Stabilized fracture fluid and crosslinker therefor |
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US (2) | US4686052A (en) |
EP (1) | EP0208373B1 (en) |
CA (1) | CA1269093A (en) |
DE (1) | DE3688303T2 (en) |
NO (1) | NO862735L (en) |
Cited By (89)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4801389A (en) * | 1987-08-03 | 1989-01-31 | Dowell Schlumberger Incorporated | High temperature guar-based fracturing fluid |
US4809783A (en) * | 1988-01-14 | 1989-03-07 | Halliburton Services | Method of dissolving organic filter cake |
US4883605A (en) * | 1987-02-09 | 1989-11-28 | E. I. Du Pont De Nemours And Company | Zirconium chelates and their use for cross-linking |
US4885103A (en) * | 1987-03-10 | 1989-12-05 | E. I. Dupont De Nemours And Company | Cross-linking titanium & zirconium chelates & their use |
DE3941337A1 (en) * | 1988-12-16 | 1990-06-21 | Tioxide Group Plc | ORGANOMETALLIC COMPOUNDS |
US5016714A (en) * | 1990-05-09 | 1991-05-21 | Halliburton Company | Biocidal well treatment method |
US5036919A (en) * | 1990-02-05 | 1991-08-06 | Dowell Schlumberger Incorporated | Fracturing with multiple fluids to improve fracture conductivity |
US5106518A (en) * | 1990-11-09 | 1992-04-21 | The Western Company Of North America | Breaker system for high viscosity fluids and method of use |
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Also Published As
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EP0208373A2 (en) | 1987-01-14 |
EP0208373A3 (en) | 1988-05-04 |
NO862735L (en) | 1987-01-09 |
NO862735D0 (en) | 1986-07-07 |
DE3688303D1 (en) | 1993-05-27 |
US4780223A (en) | 1988-10-25 |
EP0208373B1 (en) | 1993-04-21 |
CA1269093A (en) | 1990-05-15 |
DE3688303T2 (en) | 1993-07-29 |
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